CN113387710A - 一种无粘结剂的粉体造粒压片方法 - Google Patents
一种无粘结剂的粉体造粒压片方法 Download PDFInfo
- Publication number
- CN113387710A CN113387710A CN202110784891.4A CN202110784891A CN113387710A CN 113387710 A CN113387710 A CN 113387710A CN 202110784891 A CN202110784891 A CN 202110784891A CN 113387710 A CN113387710 A CN 113387710A
- Authority
- CN
- China
- Prior art keywords
- powder
- tabletting
- mixing
- binder
- sieving
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 110
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000011230 binding agent Substances 0.000 title claims abstract description 21
- 238000005469 granulation Methods 0.000 title claims abstract description 16
- 230000003179 granulation Effects 0.000 title claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 40
- 238000007873 sieving Methods 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000007580 dry-mixing Methods 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims description 23
- 238000000498 ball milling Methods 0.000 claims description 18
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 24
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000003292 glue Substances 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 2
- 230000001070 adhesive effect Effects 0.000 abstract 2
- 239000000919 ceramic Substances 0.000 description 18
- 239000000463 material Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 206010033307 Overweight Diseases 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000004677 Nylon Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910021523 barium zirconate Inorganic materials 0.000 description 1
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009475 tablet pressing Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/20—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in magnesium oxide, e.g. forsterite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
- C04B35/505—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds based on yttrium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3215—Barium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明提出了一种无粘结剂的粉体造粒压片方法，粉体不加入粘结剂混合均匀后一次过筛，然后进行煅烧再二次过筛，然后干混后得到压片粉体，接着将压片粉体使用自动压片机压片，最后升温烧结，烧结后的压片实际重量与需求重量偏差1％以下，实际尺寸与平均尺寸偏差1％以下。本发明的粉体进行多次混合，保证了原料混合的均匀性；粉体中不添加粘结剂，使得粉体纯度更高，重量更精准；一次过筛使粉体形成良好的粒度分布，煅烧、二次过筛和干混后使得不同粒度粉体分布得更为均匀，提高了压片的一致性，烧结过程中无需排胶，只需烧结使粉体进行固相反应，烧结后的片材实际重量与需求重量偏差≤1％，实际尺寸与平均尺寸偏差≤1％，制成了高精度的片材。
Description
技术领域
本发明属于材料制备技术领域，涉及一种粉体造粒方法。
背景技术
粉体压片技术广泛应用于陶瓷、玻璃生产中，是一种重要的通用技术。高重量、尺寸精度陶瓷应用广泛，包括5G陶瓷滤波器、陶瓷电容器、高精度陶瓷结构件及其他各类功能陶瓷等。玻璃制备工艺中，也会用到粉体处理、压片技术，通过控制压片重量，生产高重量精度的玻璃块材。
目前，为了获得更好的流动性，常使用粘结剂将细粒径的粉体处理为粒径增大的球形聚集体。公布号为CN111995392A的发明专利，提出了一种低成本5G基站用陶瓷滤波器粉体及其制备方法，该技术方案中使用PVA作为粘结剂造粒。授权公告号为CN102503391B的发明专利，提出了一种高铁磁性能和铁电性能的铁酸铋基复合材料的制备方法，该技术方案中，采用在粉末中加入PVA粘结剂，经60目与120目筛网过筛的方法制备所述复合材料。公布号为CN110194664A的发明专利，提出了一种石榴石结构的低介电常数微波介质陶瓷材料及制备方法，该技术方案中，采用加入PVA作为粘结剂，将混合好的粉体过100目和140目筛子的方法制备所述陶瓷材料。
粘结剂的作用主要是造粒增强粉体流动性，由于其粘性，使压制的片材更完整，不易分层缺损，但使用粘结剂，其粘结剂的纯度会影响粉体纯度，若排胶不当，易形成积碳、气孔，影响元件致密度和性能。若能不使用粘结剂，也能达到相同作用，且能制备高重量、尺寸精度的片材，这在陶瓷、玻璃生产中，将有着显著的优势。
发明内容
为解决背景技术中所述的问题，本发明提出了一种无粘结剂的粉体造粒压片方法。
该方法包括如下步骤：
步骤一、混料过筛：将粉体按配比称量混合均匀，过60-100目筛；
步骤二、煅烧：混合后粉体转移至氧化铝或石英坩埚中，升温至低于粉体熔化温度的固相反应温度，保温4-10h；
步骤三、二次过筛：将煅烧后粉体过60-100目筛；
步骤四、干混：使用混料机对二次过筛后的粉体进行干混得到压片粉体；
步骤五、压片：将压片粉体填充进模具中，使用自动压片机进行压片得到初步片材；
步骤四、烧结：初步片材转移至坩埚中，升温至烧结温度保温烧结，烧结完成后得到所需片材。
所述的步骤一中，混合方式为球磨湿混或混料机干混，过筛前需将结块粉体进行破碎使其能全部过筛。
所述的球磨湿混，采用的研磨球材质为玛瑙、氧化铝或氧化锆，球磨湿混的液体研磨介质为无水乙醇或纯水，粉体、液体研磨介质、研磨球的重量比为1:0.3-1.2:2-5，球磨机的转速为150-250r/min，研磨时间8-24h；湿混完成后烘干，烘干温度50-100℃，烘干后过10-20目筛使研磨球与粉体分离。
所述的混料机干混，混料机自转速率30-100r/min，公转速率10-60r/min，混料时间2-10h。
所述的步骤四中，混料机自转速率30-100r/min，公转速率10-60r/min，混料时间2-10h。
所述步骤五中，模具的深度依据所需片材的重量来调节，所述自动压片机为单冲自动压片机，所述压片过程的压力为10-60kN。
所述步骤六中，烧结过程的温度低于粉体熔化温度的固相反应温度，保温时间4-10h。
进一步地，步骤一中，采用的研磨球的材质为优选氧化锆。
进一步地，所用的筛网为非金属材质筛网，优选尼龙筛网。
进一步地，步骤五中，使用自动压片机压片时，模具上下模仁端面水平，每次压片时施加的压力一致，使用单冲自动压片机压片时其施加的压力的一致性更好。
更进一步地，步骤六中，所述坩埚为氧化铝坩埚或者石英坩埚。
本发明与现有技术相比，粉体进行多次混合，保证了原料混合的均匀性；粉体中不添加粘结剂，使得粉体纯度更高，重量更精准；一次过筛使粉体形成良好的粒度分布，干混使不同粒度粉体均匀分布；煅烧后使得粉体中形成一定强度的大颗粒，增强粉体流动性；二次过筛可控制煅烧后的粉体粒径，不至于过大，利于压片；通过上述处理得到的压片粉体颗粒流动性好且分布均匀，提高了压片的一致性，采用了自动压片避免人为干扰，效率高；烧结过程中无需排胶，只需烧结使粉体进行固相反应，烧结后的片材实际重量与需求重量偏差≤1％，实际尺寸与平均尺寸偏差≤1％，形成了高精度的片材。
本发明能够批量压制高重量精度、高尺寸精度的片材，可用于制备一致性优良的陶瓷及玻璃材料，工艺方法简单，实用性高。
附图说明
图1为实施例1粉体煅烧和过60目筛后的放大100倍的显微镜照片。
图2为实施例2粉体煅烧和过80目筛后的放大100倍的显微镜照片。
具体实施方式
下面结合附图详细说明本发明的实施情况，但它们并不构成对本发明的限定，仅做举例而已，同时通过说明，将更加清楚地理解本发明的优点。本领域的普通的技术人员能从本发明公开的内容直接导出或联想到的所有变形，均应认为是本发明的保护范围。实施例中其他未详细说明的部分均为现有技术。
一种无粘结剂的粉体造粒压片方法的操作步骤详细说明如下所述。
(1)混料过筛：一次混料有球磨湿混与混料机干混两种方案。对于粒度、比重差异较大的粉体，优选球磨湿混，研磨球可起到破碎作用，利于粉料粒度趋于一致。对于粒度较小且差异不大的粉体，优选混料机干混，效率更高。
若使用球磨湿混，将粉体按配比称量，加入配制好研磨球的球磨罐中，研磨罐材质为刚玉、氧化锆、玛瑙、尼龙、聚氨酯、或聚四氟乙烯，优选为聚四氟乙烯。研磨球材质为玛瑙、氧化铝、氧化锆，优选为氧化锆。再加入液体研磨介质，无水乙醇或纯水，优选为无水乙醇。粉体、液体研磨介质、研磨球重量比1:(0.3-1.2):(2-5)。无水乙醇不宜过多，混合后静置30min以上，乙醇清液不超过4mm为宜。球磨机转速150-250r/min，时间8-24h。球磨湿混完成，打开球磨罐，烘干，温度50-100℃，过10-20目筛，研磨球与粉体分离。混合后的粉体过60-100目筛，对结块粉体需进行粉碎使其全部过筛。
若使用混料机干混，混合前，粉体需全部能过100目筛，否则需粉碎使其全部过筛，粉碎方式有手动研磨、自动研磨或破碎机粉碎。干混时，混料机自转速率30-100r/min，公转速率10-60r/min，混料时间2-10h。混合完成后过60～100目筛。
(2)煅烧：将粉体转移至氧化铝或石英坩埚中，升温至低于粉体熔化温度的固相反应温度，保温4～10h。反应温度及保温时间，根据煅烧后粉体颗粒化状态确定；提高反应温度及保温时间，则粉体颗粒度更大，颗粒强度更高。这是由于常见的氧化物粉体粒度在微米级或纳米级，由于表面能影响，容易团聚，造成流动性较差，不利于压片，煅烧后使得粉体中形成一定强度的大颗粒，增强粉体流动性。
(3)二次过筛：煅烧后的粉体过60-100目筛，煅烧后的粉体易结块，需对未通过粉体进行粉碎使全部过筛，二次过筛可控制煅烧后的粉体粒径，不至于过大，利于压片。
(4)干混：过筛后不同粒径粉体分布不匀，粉体颗粒圆度不佳，使用混料机对过筛后的粉体进行干混，使不同粒径粉体分布均匀，同时，粉体碰撞、摩擦，使其球化，增强流动性。混料机自转速率30-100r/min，公转速率10-60r/min，混料时间2-10h，婚混料完成后得到压片粉体。
(5)压片：使用自动压片机压片，压片前调整模具的上下模仁端面水平，模具的直径固定后，调节模具深度以获得所需重量的片材，从而模具固定后可保证每次填充进入模具的物料重量相同，自动压片机每次压片时施加压力一致，压力范围为10-60kN，压片完成后的到初步片材。
自动压片机优选使用单冲自动压片机，其压片时施加的压力的一致性更好。根据烧结收缩比例，进行尺寸反演，可确定所需模具直径及模具深度。
(6)烧结：初步片材转移至坩埚中，升温至烧结温度保温烧结，烧结完成后得到所需片材。烧结过程的温度低于粉体熔化温度的固相反应温度，保温时间4-10h。升温速率、保温时间根据原料及片材要求设定。
烧结后，片材实际重量与需求重量偏差1％以下，实际尺寸与平均尺寸偏差1％以下。
所述筛网材质为非金属，优选为尼龙。
下面结合具体实施例对该粉体造粒压片方法进行详细说明。
实施例1
本实施例锆钛酸钡(BZT)陶瓷的化学式为BaZrxTi1-xO3，x＝0.1，其制备过程如下：
(1)混料过筛：原料为BaCO3、ZrO2、TiO2，纯度均为99.99％，按化学计量比称取步骤所需的原料，倒入球磨罐中，加入无水乙醇球磨，球磨转速200r/min，时间10h。所述原料、无水乙醇、氧化锆磨球的比值为1:0.8:2。球磨湿混完成后烘干，温度60℃，过10-20目筛，快速将研磨球与粉体分离。由于粉体烘干极易结块，使用粉碎机破碎，并使粉体全部过120目筛。
(2)煅烧：将过筛后的粉体转移至氧化铝坩埚中，5℃/min升温至1100℃，保温4h，随炉冷却，粉体颗粒化并具有一定硬度。
(3)二次过筛：煅烧后粉体易结块，过60目筛，粉碎未通过的大颗粒粉体，使其全部过筛。
(4)干混：过筛后不同粒径粉体分布不匀，粉体颗粒圆度不佳，使用混料机对过筛后的粉体进行干混。混料机自转速率60r/min，公转速率30r/min，混料时间3h。
(5)压片：使用单冲自动压片机压片，模具直径10mm，固定模具深度，可保证每次填充相同含量的物料，施加压力50kN，设定出料周期5s，可实现相同规格陶瓷坯料初步片材的连续压制。
(6)烧结：最后在1450℃下烧结10h，制成高重量、尺寸精度的BZT陶瓷。片材实际重量与需求重量偏差1％以下，实际尺寸与平均尺寸偏差1％以下。根据烧结收缩比例，进行尺寸反演，可得到需求尺寸的陶瓷。下表为制备重量240mg的BZT数据表。
表1 BZT陶瓷重量与直径数据表
实施例2
本实施例石榴石结构的微波介质陶瓷为Y3MgAl3SiO12，其制备过程如下：
(1)混料：原料为：Y2O3、MgO、Al2O3、SiO2，纯度均为99.99％，按化学计量比称取步骤所需的原料，过100目筛，将未能过筛的粉体粉碎使其全部通过。将所有粉体倒入混料机中，混料机自转速率80r/min，公转速率40r/min，混料时间6h，混合完成后过100目筛。
(2)煅烧：将过筛后的粉体转移至氧化铝坩埚中，5℃/min升温至1200℃，保温6h，随炉冷却，粉体颗粒化并具有一定硬度。
(3)二次过筛：煅烧后粉体易结块，过80目筛，粉碎未通过的大颗粒粉体，使其全部过筛。
(4)干混：过筛后不同粒径粉体分布不匀，粉体颗粒圆度不佳，使用混料机对过筛后的粉体进行干混。混料机自转速率40r/min，公转速率20r/min，混料时间2h。
(5)压片：使用单冲自动压片机压片，模具直径5mm，固定模具深度，可保证每次填充相同含量的物料，施加压力30kN，设定出料周期5s，可实现相同规格陶瓷坯料初步片材的连续压制。
(6)烧结：最后在1500℃下烧结6h，之后3℃/min降温到800℃后随炉冷却，制成高重量、尺寸精度的Y3MgAl3SiO12陶瓷。片材实际重量与需求重量偏差1％以下，实际尺寸与平均尺寸偏差1％以下。根据烧结收缩比例，进行尺寸反演，可得到需求尺寸的陶瓷。下表为制备重量80mg的Y3MgAl3SiO12数据表。
表2 Y3MgAl3SiO12陶瓷重量与直径数据表
以上结合附图及具体实施例详细描述了本发明的优选实施方式，但是，本发明并不限于上述实施方式中的具体细节，在本发明的技术构思范围内，可以对本发明的技术方案进行多种简单变型，这些简单变型均属于本发明的保护范围。
Claims (9)
1.一种无粘结剂的粉体造粒压片方法，其特征在于，包括如下步骤：
步骤一、混料过筛：将粉体按配比称量混合均匀，过60-100目筛；
步骤二、煅烧：混合后粉体转移至氧化铝或石英坩埚中，升温至低于粉体熔化温度的固相反应温度，保温4-10h；
步骤三、二次过筛：将煅烧后粉体过60-100目筛；
步骤四、干混：使用混料机对二次过筛后的粉体进行干混得到压片粉体；
步骤五、压片：将压片粉体填充进模具中，使用自动压片机进行压片得到初步片材；
步骤四、烧结：初步片材转移至坩埚中，升温至烧结温度保温烧结，烧结完成后得到所需片材。
2.根据权利要求1所述的一种无粘结剂的粉体造粒压片方法，其特征在于：所述的步骤一中，混合方式为球磨湿混或混料机干混，过筛前需将结块粉体进行破碎使其能全部过筛。
3.根据权利要求2所述的一种无粘结剂的粉体造粒压片方法，其特征在于：所述的球磨湿混中，粉体、液体研磨介质、研磨球的重量比为1:0.3-1.2:2-5，球磨机的转速为150-250r/min，研磨时间8-24h；湿混完成后烘干，烘干温度50-100℃，烘干后过10-20目筛使研磨球与粉体分离。
4.根据权利要求3所述的一种无粘结剂的粉体造粒压片方法，其特征在于：所述的球磨湿混中，采用的液体研磨介质为无水乙醇或纯水。
5.根据权利要求3所述的一种无粘结剂的粉体造粒压片方法，其特征在于：所述的球磨湿混中，采用的研磨球材质为玛瑙、氧化铝或氧化锆。
6.根据权利要求2所述的一种无粘结剂的粉体造粒压片方法，其特征在于：所述的混料机干混，混料机自转速率30-100r/min，公转速率10-60r/min，混料时间2-10h。
7.根据权利要求1-6中任意一项所述的一种无粘结剂的粉体造粒压片方法，其特征在于：所述的步骤四中，混料机自转速率30-100r/min，公转速率10-60r/min，混料时间2-10h。
8.根据权利要求1所述的一种无粘结剂的粉体造粒压片方法，其特征在于：所述步骤五中，模具的深度依据所需片材的重量来调节，所述自动压片机为单冲自动压片机，所述压片过程的压力为10-60kN。
9.根据权利要求1所述的一种粉体造粒压片方法，其特征在于：所述步骤六中，烧结过程的温度低于粉体熔化温度的固相反应温度，保温时间4-10h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110784891.4A CN113387710A (zh) | 2021-07-12 | 2021-07-12 | 一种无粘结剂的粉体造粒压片方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110784891.4A CN113387710A (zh) | 2021-07-12 | 2021-07-12 | 一种无粘结剂的粉体造粒压片方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113387710A true CN113387710A (zh) | 2021-09-14 |
Family
ID=77625827
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110784891.4A Pending CN113387710A (zh) | 2021-07-12 | 2021-07-12 | 一种无粘结剂的粉体造粒压片方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113387710A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115632131A (zh) * | 2022-11-18 | 2023-01-20 | 洲际高能科技(北京)有限公司 | 一种锂离子电池正极材料及其制备方法 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1915901A (zh) * | 2005-06-03 | 2007-02-21 | 中国科学院上海硅酸盐研究所 | 双掺杂的钇铝石榴石透明陶瓷材料及制备方法 |
| CN101665356A (zh) * | 2009-07-24 | 2010-03-10 | 中国科学院上海光学精密机械研究所 | 掺锆氧化钇基透明陶瓷及其制备方法 |
| CN106457203A (zh) * | 2014-04-25 | 2017-02-22 | 艾拉梅公司 | 在无粘结剂下制备吸附材料的包括水热处理步骤的方法及用该材料从盐水溶液中提取锂的方法 |
| CN106747440A (zh) * | 2016-12-22 | 2017-05-31 | 桂林电子科技大学 | 一种可见光透明储能陶瓷及其制备方法 |
-
2021
- 2021-07-12 CN CN202110784891.4A patent/CN113387710A/zh active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1915901A (zh) * | 2005-06-03 | 2007-02-21 | 中国科学院上海硅酸盐研究所 | 双掺杂的钇铝石榴石透明陶瓷材料及制备方法 |
| CN101665356A (zh) * | 2009-07-24 | 2010-03-10 | 中国科学院上海光学精密机械研究所 | 掺锆氧化钇基透明陶瓷及其制备方法 |
| CN106457203A (zh) * | 2014-04-25 | 2017-02-22 | 艾拉梅公司 | 在无粘结剂下制备吸附材料的包括水热处理步骤的方法及用该材料从盐水溶液中提取锂的方法 |
| CN106747440A (zh) * | 2016-12-22 | 2017-05-31 | 桂林电子科技大学 | 一种可见光透明储能陶瓷及其制备方法 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115632131A (zh) * | 2022-11-18 | 2023-01-20 | 洲际高能科技(北京)有限公司 | 一种锂离子电池正极材料及其制备方法 |
| CN115632131B (zh) * | 2022-11-18 | 2024-05-10 | 洲际高能科技(北京)有限公司 | 一种锂离子电池正极材料及其制备方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103130499B (zh) | 一种微波介质陶瓷材料的制备方法 | |
| CN100551877C (zh) | 一种三元锂陶瓷微球的冷冻成型制备方法 | |
| CN110128129A (zh) | 一种低损耗石榴石铁氧体材料的制备方法 | |
| CN106365651B (zh) | 球形骨料增强耐火材料的制备方法 | |
| CN111423229B (zh) | 管状ito靶材坯体烧结用同步收缩衬管及其制备方法 | |
| CN111495513B (zh) | 一种干法研磨活性α-氧化铝微粉的助磨剂及其应用 | |
| CN101648814A (zh) | 一步固相反应法制备高性能陶瓷的方法 | |
| CN103172367A (zh) | 一种微波介质陶瓷材料的制备方法 | |
| CN104860672A (zh) | 一种高介微波陶瓷介质材料及其制备方法 | |
| CN105801112A (zh) | Nd、Al共掺杂取代Ba0.4Sr0.6TiO3巨介电陶瓷及其制备方法 | |
| CN104909725A (zh) | 一种无指甲纹缺陷的氧化铝瓷球制备方法 | |
| CN100494117C (zh) | 一种低介电损耗CaCu3Ti4O12陶瓷的制备方法 | |
| WO2023093221A1 (zh) | 一种高稳定低损耗的微波介质陶瓷材料的制备方法及应用其制得的微波介质陶瓷材料 | |
| CN111004030B (zh) | 一种MgTiO3基微波介质陶瓷及其制备方法 | |
| CN113387710A (zh) | 一种无粘结剂的粉体造粒压片方法 | |
| CN104844195A (zh) | 一种制备钛酸铜铋钠陶瓷的方法 | |
| CN103833392A (zh) | 一种烧结刚玉的制备方法 | |
| CN106747435B (zh) | 一种温度稳定的芯-壳结构微波介质陶瓷的制备方法 | |
| CN104944940A (zh) | 一种温度稳定型钛酸镁基微波介质陶瓷及其制备方法 | |
| CN113744991A (zh) | 一种Co2Z型铁氧体材料及其制备方法和用途 | |
| CN109020542A (zh) | 中介电常数超高品质因数微波介质陶瓷的制备方法 | |
| CN111908897B (zh) | MgO基微波陶瓷介质材料及其制备方法 | |
| CN113121214A (zh) | 一种石墨尾矿基微波介质陶瓷材料及其制备方法 | |
| CN115304367B (zh) | 一种微波介电陶瓷的制备方法和产品 | |
| CN107879735B (zh) | 一种中高温低膨胀系数镁橄榄石-锂辉石复合陶瓷材料的制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210914 |
|
| RJ01 | Rejection of invention patent application after publication |